Edexcel International Chemistry

A-level

Practical 15
Analysis of Some Inorganic and Organic
Unknowns

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These notes are a summary of chemical tests needed for both Unit 3
(practical 8) and Unit 6 (practical 15).

Inorganic

Test for acid or base

● Use litmus paper
○ Blue litmus paper turns ​red ​= acid
○ Red litmus paper turns ​blue ​= base
● Use universal indicator and compare to a scale like the one below

Flame tests for Group I and Group II metal cations

Method:
● To clean the nichrome wire - dip the wire in a solution of concentrated HCl and then
into a Bunsen burner flame.
● Dip the wire into the unknown compound and carefully place it at the top of the blue
Bunsen burner flame.
● Observe the colour:
○ Li​+​ = ​red
○ Na​+​ = ​orange/​yellow
○ K​+​ = ​lilac
○ Rb​+​ = ​red
○ Cs​+​ = ​blue
○ Mg​2+​ = no colour
○ Ca​2+​ = ​brick-red
○ Sr​2+​ = ​crimson red
○ Ba​2+​ =​ green

Test for NH​4​+​ ions

● Add aqueous NaOH and gently warm the mixture.
● The ammonia gas will turn moist pH indicator paper blue.
● Additionally, a pungent smell is given off.

Test for SO​4​2​−​ ions

● Add acidified barium chloride solution.
● White ppt forms (BaSO​4​).

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Mixtures of anions
When carrying out the above test, it may be useful to add some HNO​3 before you add
Ba​2+​(aq)​.The carbonate anion also gives a white precipitate with barium cations, and addition
of acid will remove any carbonates present in the mixture. Then, the test for sulfates can be
conducted.

Halides
● Dissolve 2 spatulas of the unknown product in 10 cm​3​ of water.
● Then, add a few drops of dilute nitric acid and silver nitrate solution. Observe the
colour of any precipitate formed:
○ Cl​−​ forms a white ppt with silver nitrate which is soluble in dilute NH​3​.
○ Br​−​ forms a cream ppt with silver nitrate which is soluble in concentrated NH​3​.
○ I​−​ forms yellow ppt with silver nitrate which is insoluble in NH​3​.
● The colours are all quite similar, so the solubility test with ammonia is a good way to
confirm the identity of the halide ion present.

Halides can also be tested for by reacting a solid halide salt with conc. H​2​SO​4​.
● Chloride produces steamy fumes of HCl.
● Bromide produces steamy fumes, brown vapour (HBr, Br​2​, SO​2​).
● Iodide produces steamy fumes, purple vapours, black solid (I​2​, HI, SO​2 or even solid
S).

Metal cations

Testing for various metal cations using sodium hydroxide. Group I hydroxides are all soluble.
Metal cation add some NaOH add more NaOH

Mg​2+ White suspension n/a

Ca​2+ White suspension, but more soluble than n/a

Mg(OH)​2

Sr​2+​, Ba​2+ Soluble hydroxides. n/a

Zn​2+ White ppt, Zn(OH)​2​. Soluble in NH​3​, Ppt dissolves, colourless

colourless solution, Zn(NH​3​)​4​2+ solution, Zn(OH)​4​2​−

Al​3+ White ppt, Al(OH)​3 Ppt dissolves, colourless

solution, Al(OH)​4​−

Ag​+ Dark brown ppt, Ag​2​O. Ppt doesn’t dissolve

Soluble in NH​3​, colourless solution, Ag(NH​3​)​2​+

Cu​2+ Blue ppt, Cu(H​2​O)​4​(OH)​2​, soluble in excess Ppt doesn’t dissolve

NH​3 to
​ form a deep blue solution, Cu(NH​3​)​4​2+

Fe​3+ Brown ppt, Fe(OH)​3 Ppt doesn’t dissolve

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 Fe​2+ White/green ppt, slowly turning brown when
exposed to air (oxidation to Fe(OH)​3​) Ppt doesn’t dissolve

Cr​3+​ (green
​ or Blue-green ppt, Cr(H​2​O)​3​(OH)​3​, soluble in Ppt dissolves, Cr(OH)​6​3−
blue) NH​3​, Cr(NH​3​)​6​3+​, violet solution green solution.

Co​2+ Blueish ppt, Co(H​2​O)​4​(OH)​2​. Slowly turns

pink. The precipitate dissolves in NH​3​,
Co(NH​3​)​6​2+​, light brown colour. Turns to dark
brown upon standing - slow oxidation to Ppt doesn’t dissolve
Co(III).

Ni​2+ Green ppt, Ni(H​2​O)​4​(OH)​2​. Soluble in NH​3​ -

blue solution, Ni(NH​3​)​6​2+ Ppt doesn’t dissolve

Mn​2+​ (pale Off-white ppt, Mn(OH)​2​ turns brown upon Ppt doesn’t dissolve
pink) exposure to air (oxidation to MnO​2​)

Transition metal colours

● MnO​4​−​ = violet
● CrO​4​2−​ = yellow (could be converted to orange Cr​2​O​7​2−​ in acid and vice versa).

Test for bromide

● Add chlorine water to a solution of bromides
● Produces an orange solution if present.
● ​ me effervescence may be observed.
So

Organic

Haloalkanes
See core practical 5, hydrolysis followed by halide test.

Alkenes
● Add 10 drops of your compound to a test tube followed by 1 cm​3 of bromine water
and shake.
● If there are any C=C bonds, the colour change occurs from orange to colourless.

Alcohols
Alcohols can be primary, secondary or tertiary. Primary and secondary alcohols can be
oxidised to aldehydes and ketones respectively but tertiary alcohols cannot be oxidised.
● Add 1 cm​3 of your unknown compound to a pear shaped flask followed by 5 cm​3 of
acidified potassium dichromate solution.
● Heat the mixture under distillation conditions so the product is collected.
● If there is a colour change from ​orange ​to ​green ​then the potassium dichromate has
been reduced meaning a primary or secondary alcohol is present, these will have

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 formed aldehydes and ketones respectively. Tollen’s reagent or Fehling’s solution
can then be used to determine if the alcohol was primary or secondary.
● If there is no colour change, a tertiary alcohol was present.

Test for CO​3​2-​ and HCO​3​- ​ions

● Add aqueous acid.
● If CO​3​2-​ or HCO​3​-​ ions are present bubbles of CO​2​ gas will be observed.
● Use a delivery tube to pass the CO​2​ through limewater.
● The solution will turn cloudy due to formation of CaCO​3​ precipitate.

Carboxylic acid
● Add 1 cm​3 each of the unknown substance and ethanol into a boiling tube and heat
for 5 minutes in a beaker of boiling water.
● Add a few drops of sodium carbonate solution.
● If a carboxylic acid was present there will be a sweet ester smell.

Aldehydes and Ketones

Using Tollens’ solution

● Add 10 drops of the unknown compound to a test tube followed by 5 cm​3 of ethanol,
5 cm​3​ of sodium hydroxide solution and warm in a water bath for 5-10 minutes.
● Then add 1 cm​3​ of dilute nitric acid solution and 10 drops of silver nitrate solution.
● Aldehydes give a positive test and a silver mirror is observed.
● Ketones cannot be oxidised, so no change observed

Using Fehling’s reagent

● Add 1 cm​3 of blue Fehling’s reagent to 10 drops of the unknown compound and warm
the mixture in a 60 °C water bath
● Aldehydes give a positive test and form a brick red precipitate.
● Ketones don’t react so the solution stays deep blue.

Iodoform reaction
● Warm with iodine and sodium hydroxide.
● Yellow precipitate.
● Antiseptic smell (triiodomethane, iodoform).
● Positive test with methyl ketones (e.g. propanone), ethanal, ethanol, and methyl
secondary alcohols (e.g. propan-2-ol).

Esterification test
● Gently warm an alcohol and a carboxylic acid in the presence of concentrated H​2​SO​4
● Should produce a compound with a characteristic smell, (e.g. pineapples).

Solubility test:
● Compounds with groups that can form H-bonds may be soluble in water, (e.g.
amines, alcohols, carboxylic acids etc.)

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● Some carboxylic acids may not be soluble in water, but may be soluble in alkaline
solution (due to formation of RCOO​−​).
● Same goes with amines. Some may not be soluble in water, but will be soluble in
acidic solution (e.g. formation of RNH​3​+​).

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